CN113270242A - All-inorganic high-temperature-resistant composite magnetic powder core and preparation method thereof - Google Patents

All-inorganic high-temperature-resistant composite magnetic powder core and preparation method thereof Download PDF

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CN113270242A
CN113270242A CN202110407003.7A CN202110407003A CN113270242A CN 113270242 A CN113270242 A CN 113270242A CN 202110407003 A CN202110407003 A CN 202110407003A CN 113270242 A CN113270242 A CN 113270242A
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magnetic powder
powder core
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张雪峰
李红霞
刘先国
李忠
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Hangzhou Dianzi University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147Alloys characterised by their composition
    • H01F1/14766Fe-Si based alloys
    • H01F1/14791Fe-Si-Al based alloys, e.g. Sendust
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets

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Abstract

本发明涉及磁性元器件技术领域,尤其涉及一种全无机耐高温复合磁粉芯及其制备方法,包括以下步骤:(1)将FeSiAl金属软磁粉加入到NaAlO2和(NaPO3)6的混合溶液中,加热搅拌均匀,烘干,完成绝缘包覆;(2)加入复合粘结剂,和润滑剂,压制成型,得复合磁粉芯坯体;所述复合粘结剂为NaOH和Na2SiO3的混合物;(3)将步骤(2)得到的复合磁粉芯坯体在真空或惰性气体或还原气氛中进行热处理,冷却,喷涂,即得全无机耐高温复合磁粉芯。本发明制得的全无机耐高温复合磁粉芯具有包覆层厚度可控,损耗低、磁导率高和耐高温的特点。The invention relates to the technical field of magnetic components, in particular to an all-inorganic high temperature resistant composite magnetic powder core and a preparation method thereof, comprising the following steps: (1) adding FeSiAl metal soft magnetic powder to a mixed solution of NaAlO 2 and (NaPO 3 ) 6 In the process, heating and stirring evenly, drying to complete the insulation coating; (2) adding a composite binder and lubricant, and pressing and molding to obtain a composite magnetic powder core blank; the composite binder is NaOH and Na 2 SiO 3 (3) Heat treatment, cooling and spraying of the composite magnetic powder core blank obtained in step (2) in vacuum or inert gas or reducing atmosphere to obtain an all-inorganic high temperature resistant composite magnetic powder core. The all-inorganic high temperature resistant composite magnetic powder core prepared by the invention has the characteristics of controllable coating thickness, low loss, high magnetic permeability and high temperature resistance.

Description

All-inorganic high-temperature-resistant composite magnetic powder core and preparation method thereof
Technical Field
The invention relates to the technical field of magnetic components, in particular to an all-inorganic high-temperature-resistant composite magnetic powder core and a preparation method thereof.
Background
The sendust/sendust magnetic powder core is widely applied to the fields of communication, uninterruptible power supplies, solid laser power supplies, photovoltaic power generation systems and the like because of high saturation magnetic induction intensity and relatively low loss. The sendust/sendust material has power loss in an alternating magnetic field and is dominated by eddy current loss at high frequency. The eddy current among the particles can be blocked by insulating and coating the magnetic powder particles, and the eddy current loss of the magnetic powder core is reduced, so that the iron-silicon-aluminum/iron-silicon magnetic powder core with high magnetic conductivity and low loss is obtained.
The use of organic polymers as insulating agents and binders has been commercialized. The organic resin is adopted to coat the magnetic powder particles, so that the resistivity of the powder core can be obviously improved, and the loss of the magnetic powder core can be reduced. More importantly, the organic polymer has poor high temperature resistance, the general heat-resistant temperature is not more than 500 ℃, and the conventional heat treatment temperature can reach 600-800 ℃.
In recent years, inorganic insulating agents such as phosphates and ceramic oxide coatings have received much attention and have been under some progress. However, the chemical stability and structural stability of the phosphated coating are poor, and as the annealing temperature increases, the coating insulation decreases, resulting in increased losses. When ceramic oxide is adopted for coating, the material can withstand higher heat treatment temperature, but the adhesion between the oxide coating layer and the powder core is poor, so that good insulating coating is difficult to form on the surface of the powder core, meanwhile, the thickness of the oxide coating layer is difficult to control, the thickness of the insulating coating layer is difficult to control on a nanometer scale, and along with the increase of the thickness of the insulating coating material, the air gap rate inside the powder core is increased, so that the magnetic permeability of the magnetic powder core can be reduced. More importantly, the excessive oxide coating can lead to uneven insulation coating, the powder core is easy to crack in the compression molding process, and the eddy current loss of the magnetic core is increased. Therefore, how to select a proper all-inorganic coating material and a proper coating thickness is a great challenge to realize a high-permeability and low-loss powder core.
Chinese patent literature discloses a ferrite composite magnetic powder core and a preparation method thereof, the application publication number of which is CN103426584A, and the invention adopts nickel-zinc ferrite nano particles prepared by a hydrothermal method to coat magnetic powder to prepare the novel nickel-zinc ferrite composite magnetic powder core. However, in this patent, the ferrite and the magnetic powder are in solid-solid contact, so that the wettability is poor, and it is difficult to form a good coating. In addition, the values of permeability and loss of the product are not mentioned in this patent either.
Chinese patent literature discloses an inorganic insulating binder for a metal soft magnetic powder core, the application publication number of which is CN101089108A, the inorganic insulating binder of the invention is made of SiO2、Al2O3、ZrO2Mica powder and water, and has the double effects of insulation and bonding. However, the ceramic oxide and other materials used in the patent are insoluble in water, and it is difficult to obtain an aqueous solution with uniform distribution, so that the uniformity and thickness of the insulating binder coated on the surface of the magnetic powder are difficult to control, the Q value is low, and the loss is increased.
The Chinese patent literature discloses a method for coating and bonding a metal magnetic powder core by using inorganic gel, the application publication number of the method is CN109616273A, the coating agent of the method is one or two of magnesium aluminum silicate, saponite, bentonite and montmorillonite, and the binder is attapulgite. The inorganic gel coating layer is high temperature resistant, and reduces the cost and loss of the magnetic powder core. However, in the patent, because the particle sizes of the magnesium aluminum silicate, the attapulgite and the like are in the micron order, the uniform distribution in the gel is difficult to realize, and the gel has poor fluidity in the magnetic powder and can generate an agglomeration phenomenon. Meanwhile, the gaps between large particles are difficult to fill, so that the magnetic permeability is reduced. Moreover, the metal magnetic powder needs to be passivated and treated, which increases the preparation cost.
Based on the above problems, it is significant to design a new all-inorganic high temperature resistant insulating coating agent to simultaneously realize high magnetic permeability and low loss of the metal magnetic powder core.
Disclosure of Invention
The invention provides a preparation method of an all-inorganic high-temperature-resistant composite magnetic powder core, which aims to solve the problems of uncontrollable coating layer thickness, easy cracking, low magnetic powder core magnetic conductivity, high loss and poor high-temperature resistance of the existing magnetic powder core insulation coating process, and has the advantages of low cost, simple operation and easy large-scale production.
The invention also provides the all-inorganic high-temperature-resistant composite magnetic powder core prepared by the preparation method, and the magnetic powder core has the characteristics of controllable coating thickness, low loss, high magnetic conductivity and high temperature resistance.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an all-inorganic high-temperature-resistant composite magnetic powder core comprises the following steps:
(1) adding FeSiAl metal soft magnetic powder into NaAlO2And (NaPO)3)6Heating and stirring the mixed solution uniformly, and drying to finish insulating coating; NaAlO2And (NaPO)3)6The mixed solution has good fluidity and wettability, and NaAlO is controlled2And (NaPO)3)6The proportion of (A) can be regulated and controlled, and Al (OH) generated by hydrolysis3The FeSiAl soft magnetic powder can be uniformly and compactly coated on the outer surface of the FeSiAl soft magnetic powder; the concentration and the dosage of the mixed solution can be controlled, and the final Al can be controlled on the nanometer scale2O3The thickness of the coating layer effectively prevents the coating layer from cracking, improves the resistivity of the magnetic powder core and reduces the loss;
(2) adding a composite binder into the FeSiAl metal soft magnetic powder subjected to the insulation coating treatment in the step (1), fully stirring, keeping the temperature at 90-100 ℃ for 20-40 min, drying, adding a lubricant, and performing compression molding to obtain a composite magnetic powder core blank; the composite binder is NaOH and Na2SiO3A mixture of (a); using NaOH and Na2SiO3The mixture is used as a composite binder, and the composite binder has good adhesiveness and high temperature resistance, and can prevent the device from losing effect in high-temperature use
(3) And (3) carrying out heat treatment on the composite magnetic powder core blank obtained in the step (2) in vacuum or inert gas or reducing atmosphere, cooling and spraying to obtain the all-inorganic high-temperature-resistant composite magnetic powder core. Al (OH) coated on the outer surface of the FeSiAl metal soft magnetic powder in the heat treatment process3Decomposition to Al2O3Nanoparticles, Al while achieving coating2O3The nanoparticles can be filled in the large particles and the large particles in the magnetic powder coreThe micro-gaps between the particles reduce the gap degree, increase the density of the powder core and obtain higher magnetic conductivity.
Preferably, in the step (1), the NaAlO is based on the total mass of the FeSiAl metal soft magnetic powder2And (NaPO)3)6The mixed solution of (A) comprises 0.05-3 wt% of NaAlO20.01 to 0.08wt% (NaPO)3)6And 10 to 15wt% of water. The final Al can be controlled on the nanometer level by adjusting the concentration and the dosage of the aqueous solution2O3The thickness of the coating layer effectively prevents the coating layer from cracking, improves the resistivity of the magnetic powder core and reduces the loss.
Preferably, the NaAlO2And (NaPO)3)6The mixed solution of (A) comprises 0.1-2 wt% of NaAlO20.02 to 0.05wt% (NaPO)3)6
NaAlO2And (NaPO)3)6The aqueous solution has good fluidity and wettability by controlling NaAlO2And (NaPO)3)6The hydrolysis reaction can be regulated and controlled. Al (OH) formed by hydrolysis3Can be uniformly and compactly coated outside the magnetic powder core and decomposed into Al in the subsequent thermal annealing treatment process2O3Nanoparticles, Al while achieving coating2O3The nano particles can fill micro gaps between large particles in the magnetic powder core, so that the gap degree is reduced, the density of the powder core is increased, and higher magnetic conductivity is obtained.
Preferably, the heating temperature is 80-100 ℃, and the drying temperature is 90-120 ℃.
Preferably, in the step (2), the composite binder is 0.5-5 wt% of Na based on the total mass of the FeSiAl metal soft magnetic powder2SiO3And 0.002-0.02 wt% of NaOH.
Preferably, the composite binder consists of 1-3 wt% of Na2SiO3And 0.005-0.015 wt% of NaOH. .
Preferably, in the step (2), the lubricant is added in an amount of 0.5 to 1.0 wt% based on the total mass of the FeSiAl metal soft magnetic powder.
Preferably, in the step (2), the lubricant is one or two of zinc stearate and barium stearate.
Preferably, in the step (3), the heat treatment temperature is 600-780 ℃ and the time is 0.5-2 h.
An all-inorganic high-temperature-resistant composite magnetic powder core prepared by the preparation method.
Therefore, the invention has the following beneficial effects:
(1) the coating agent used by the invention is water-soluble, has good fluidity and wettability, and can realize uniform and compact coating of the magnetic powder core, thereby improving the resistivity of the magnetic powder core and reducing the power loss; the preparation method is simple, has low cost and no pollution to the environment, and is suitable for mass production;
(2) the all-inorganic high-temperature-resistant composite magnetic powder core prepared by the preparation method has the characteristics of controllable coating layer thickness, low loss, high magnetic conductivity and high temperature resistance.
Detailed Description
The technical solution of the present invention is further specifically described below by way of specific examples.
In the present invention, all the equipment and materials are commercially available or commonly used in the art, and the methods in the following examples are conventional in the art unless otherwise specified.
Example 1
(1) Adding FeSiAl metal soft magnetic powder into NaAlO2And (NaPO)3)6Heating and stirring the mixed solution at 80 ℃ for 30min until the mixed solution is uniformly mixed, and drying the mixed solution at 100 ℃ to finish insulating coating; the NaAlO is based on the total mass of the FeSiAl metal soft magnetic powder2And (NaPO)3)6The mixed solution of (A) contains 0.1 wt% of NaAlO20.02wt% of (NaPO)3)6And 10 wt% water; NaAlO is added2Dissolving in deionized water and adding (NaPO)3)6Adding, magnetically stirring for 30 minutes to obtain a colorless transparent solution for later use;
(2) after the step (1) of insulating coatingAdding a composite binder into the treated FeSiAl metal soft magnetic powder, fully stirring, and drying at 95 ℃ for 30 min; then adding zinc stearate accounting for 0.5 wt% of the total mass of the FeSiAl metal soft magnetic powder, and performing compression molding under 1500MPa to obtain a composite magnetic powder core blank with the outer diameter of 33.00mm, the inner diameter of 19.90mm and the height of 10.7 mm; the composite binder is composed of 1 wt% of Na2SiO3And 0.01 wt% NaOH;
(3) and (3) carrying out heat treatment on the composite magnetic powder core blank obtained in the step (2) at the temperature of 700 ℃ in vacuum for 45min, cooling and spraying to obtain the all-inorganic high-temperature-resistant composite magnetic powder core.
Example 2
(1) Adding FeSiAl metal soft magnetic powder into NaAlO2And (NaPO)3)6Heating and stirring the mixed solution at 100 ℃, and drying the mixed solution at 90 ℃ to finish insulating coating; the NaAlO is based on the total mass of the FeSiAl metal soft magnetic powder2And (NaPO)3)6The mixed solution of (A) contains 0.2 wt% of NaAlO20.02wt% of (NaPO)3)6And 10 wt% water;
(2) adding a composite binder into the FeSiAl metal soft magnetic powder subjected to the insulation coating treatment in the step (1), fully stirring, keeping the temperature at 90 ℃ for 40min, drying, adding zinc stearate accounting for 0.8 wt% of the total mass of the FeSiAl metal soft magnetic powder and barium stearate accounting for 0.2 wt% of the total mass of the FeSiAl metal soft magnetic powder, and performing compression molding under the pressure of 1800MPa to obtain a composite magnetic powder core blank with the outer diameter of 33.00mm, the inner diameter of 19.90mm and the height of 10.7 mm; the composite binder consists of 2wt% of Na2SiO3And 0.01 wt% NaOH;
(3) and (3) carrying out heat treatment on the composite magnetic powder core blank obtained in the step (2) in nitrogen at the temperature of 600 ℃ for 2h, cooling and spraying to obtain the all-inorganic high-temperature-resistant composite magnetic powder core.
Example 3
(1) Adding FeSiAl metal soft magnetic powder into NaAlO2And (NaPO)3)6Heating and stirring the mixed solution at 90 ℃, and drying the mixed solution at 120 ℃ to finish insulating coating; the NaAlO is based on the total mass of the FeSiAl metal soft magnetic powder2And (NaPO)3)6The mixed solution of (1) includes 0.3wt% NaAlO20.02wt% of (NaPO)3)6And 10 wt% water;
(2) adding a composite binder into the FeSiAl metal soft magnetic powder subjected to the insulation coating treatment in the step (1), fully stirring, keeping the temperature at 100 ℃ for 20min, drying, adding barium stearate accounting for 0.8 wt% of the total mass of the FeSiAl metal soft magnetic powder, and performing compression molding under the pressure of 2000MPa to obtain a composite magnetic powder core blank with the outer diameter of 33.00mm, the inner diameter of 19.90mm and the height of 10.7 mm; the composite binder is composed of 3wt% of Na2SiO3And 0.01 wt% NaOH;
(3) and (3) carrying out heat treatment on the composite magnetic powder core blank obtained in the step (2) in hydrogen at the temperature of 780 ℃ for 0.5h, cooling and spraying to obtain the all-inorganic high-temperature-resistant composite magnetic powder core.
The magnetic powder cores prepared in examples 1 to 3 were subjected to performance tests, and the results are shown in the following table:
Figure BDA0003022735880000051
the coating process adopted by the invention ensures that the magnetic powder coating layer is thin, uniform and compact, the magnetic conductivity is high, and the loss is greatly reduced. The invention is easy for scale production and has good application prospect.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.

Claims (10)

1.一种全无机耐高温复合磁粉芯的制备方法,其特征在于,包括以下步骤:1. a preparation method of all-inorganic high temperature resistant composite magnetic powder core, is characterized in that, comprises the following steps: (1)将FeSiAl金属软磁粉加入到NaAlO2和(NaPO3)6的混合溶液中,加热搅拌均匀,烘干,完成绝缘包覆;(1) Add FeSiAl metal soft magnetic powder into the mixed solution of NaAlO 2 and (NaPO 3 ) 6 , heat and stir evenly, and dry to complete the insulation coating; (2)在经过步骤(1)绝缘包覆处理后的FeSiAl金属软磁粉中加入复合粘结剂,和润滑剂,压制成型,得复合磁粉芯坯体;所述复合粘结剂为NaOH和Na2SiO3的混合物;(2) Adding a composite binder and a lubricant to the FeSiAl metal soft magnetic powder after the insulation coating treatment in step (1), and pressing and molding to obtain a composite magnetic powder core blank; the composite binders are NaOH and Na 2 a mixture of SiO 3 ; (3)将步骤(2)得到的复合磁粉芯坯体在真空或惰性气体或还原气氛中进行热处理,冷却,喷涂,即得全无机耐高温复合磁粉芯。(3) The composite magnetic powder core body obtained in step (2) is heat-treated in a vacuum or in an inert gas or reducing atmosphere, cooled and sprayed to obtain an all-inorganic high temperature resistant composite magnetic powder core. 2.根据权利要求1所述的制备方法,其特征在于,步骤(1)中,以FeSiAl金属软磁粉总质量为基准,所述NaAlO2和(NaPO3)6的混合溶液中包括0.05~3wt%的NaAlO2、0.01~0.08wt%的(NaPO3)6和10~15wt%的水。2 . The preparation method according to claim 1 , wherein in step (1), based on the total mass of FeSiAl metal soft magnetic powder, the mixed solution of NaAlO 2 and (NaPO 3 ) 6 includes 0.05 to 3 wt. % NaAlO 2 , 0.01~0.08wt% (NaPO 3 ) 6 and 10~15wt% water. 3.根据权利要求2所述的制备方法,其特征在于,所述NaAlO2和(NaPO3)6的混合溶液中包括0.1~2wt%的NaAlO2和0.02~0.05wt%的(NaPO3)63. preparation method according to claim 2, is characterized in that, the mixed solution of described NaAlO 2 and (NaPO 3 ) 6 includes 0.1~2wt% NaAlO 2 and 0.02~0.05wt% (NaPO 3 ) 6 . 4.根据权利要求1所述的制备方法,其特征在于,步骤(1)中,加热温度为80~100oC,烘干温度为90~120 oC。4. The preparation method according to claim 1, characterized in that, in step (1), the heating temperature is 80-100 ℃, and the drying temperature is 90-120 ℃ . 5.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,以FeSiAl金属软磁粉总质量为基准,所述复合粘结剂由0.5~5wt%的Na2SiO3和0.002~0.02wt%的NaOH组成。5 . The preparation method according to claim 1 , wherein in step (2), based on the total mass of FeSiAl metal soft magnetic powder, the composite binder is composed of 0.5-5wt% Na 2 SiO 3 and 0.002 ~0.02 wt% NaOH composition. 6.根据权利要求5所述的制备方法,其特征在于,所述复合粘结剂由1~3wt%的Na2SiO3和0.005~0.015wt%的NaOH组成。6 . The preparation method according to claim 5 , wherein the composite binder is composed of 1-3wt% Na 2 SiO 3 and 0.005-0.015wt% NaOH. 7 . 7.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,以FeSiAl金属软磁粉总质量为基准,所述润滑剂的添加量为0.5~1.0wt%;所述润滑剂为硬脂酸锌和硬脂酸钡中的一种或两种。7 . The preparation method according to claim 1 , wherein in step (2), the lubricant is added in an amount of 0.5-1.0 wt % based on the total mass of FeSiAl metal soft magnetic powder; It is one or both of zinc stearate and barium stearate. 8.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,压制成型的压强为1500~2000 MPa。8 . The preparation method according to claim 1 , wherein, in step (2), the pressure of pressing is 1500-2000 MPa. 9 . 9.根据权利要求1所述的制备方法,其特征在于,步骤(3)中,热处理温度为600~780℃,时间为0.5~2 h。9 . The preparation method according to claim 1 , wherein in step (3), the heat treatment temperature is 600-780° C., and the time is 0.5-2 h. 10 . 10.一种如权利要求1-9任一所述的制备方法制得的全无机耐高温复合磁粉芯。10. An all-inorganic high temperature resistant composite magnetic powder core prepared by the preparation method according to any one of claims 1-9.
CN202110407003.7A 2021-04-15 2021-04-15 All-inorganic high-temperature-resistant composite magnetic powder core and preparation method thereof Withdrawn CN113270242A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
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CN116825468A (en) * 2023-08-04 2023-09-29 广东泛瑞新材料有限公司 Iron-cobalt magnetic core and preparation method and application thereof
CN116833407A (en) * 2023-05-09 2023-10-03 中南大学 Soft magnetic composite material and preparation method thereof
CN118173371A (en) * 2024-04-22 2024-06-11 国网智能电网研究院有限公司 A kind of soft magnetic powder core with high anti-saturation ability and its preparation method and application

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116833407A (en) * 2023-05-09 2023-10-03 中南大学 Soft magnetic composite material and preparation method thereof
CN116833407B (en) * 2023-05-09 2024-03-01 中南大学 Soft magnetic composite material
CN116825468A (en) * 2023-08-04 2023-09-29 广东泛瑞新材料有限公司 Iron-cobalt magnetic core and preparation method and application thereof
CN116825468B (en) * 2023-08-04 2024-01-12 广东泛瑞新材料有限公司 Iron-cobalt magnetic core and preparation method and application thereof
CN118173371A (en) * 2024-04-22 2024-06-11 国网智能电网研究院有限公司 A kind of soft magnetic powder core with high anti-saturation ability and its preparation method and application

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Application publication date: 20210817